Institute of Agricultural Quality Standards and Testing Technology Research/Hubei Key Laboratory of Nutritional Quality and Safety of Agro products, Hubei Academy of Agricultural Sciences, Wuhan, 430064, China.
Institute of Agricultural Quality Standards and Testing Technology Research/Hubei Key Laboratory of Nutritional Quality and Safety of Agro products, Hubei Academy of Agricultural Sciences, Wuhan, 430064, China.
J Chromatogr A. 2020 Dec 20;1634:461645. doi: 10.1016/j.chroma.2020.461645. Epub 2020 Oct 27.
In current study, a rapid and sensitive method for simultaneous determination of 8 phenoxy carboxylic acid (PCA) herbicides in environmental water samples was established based on an octyl and amino functionalized magnetic mesoporous silica (mOAS). The mOAS sorbent was fabricated by simple modification of octyl and aminopropyl groups onto the surface of magnetic mesoporous silica. Various techniques were employed to characterize the physical and chemical properties of the mOAS sorbent. The mOAS sorbent showed good extraction capacity and selectivity for PCA herbicides owing to the mixed-mode hydrophobic and ionic exchange interaction mechanisms. Then a one-factor-at-a-time approach was utilized for the optimization of extraction, washing and eluting conditions. Under the optimum conditions, wide linearity ranges with squared correlation coefficients ranging from 0.9888 to 0.9966 were obtained, and the method detection of limits (LODs) were in the range of 0.005-0.02 ng/mL. Furthermore, recoveries ranged from 86.9 to 114.6% with intra- and inter-day relative standard deviation (RSD) of 0.8-11.0% at three concentration levels spiked in blank water sample. Finally, the as-proposed method was successfully applied to extract 8 PCA herbicides in real water samples followed by determination with ultra-high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS). Results showed that the mOAS as adsorbent for magnetic solid phase extraction (MSPE) of acidic herbicides is an efficient alternative with simplicity and rapidity.
在当前的研究中，基于辛基和氨基功能化的磁性介孔硅（mOAS），建立了一种快速灵敏的同时测定环境水样中 8 种苯氧羧酸（PCA）除草剂的方法。mOAS 吸附剂是通过将辛基和氨丙基基团简单修饰到磁性介孔硅表面而制备的。采用多种技术对 mOAS 吸附剂的物理化学性质进行了表征。由于混合模式的疏水和离子交换相互作用机制，mOAS 吸附剂对 PCA 除草剂具有良好的萃取能力和选择性。然后，采用单因素法优化萃取、洗涤和洗脱条件。在最佳条件下，得到了线性范围较宽的结果，相关系数平方从 0.9888 到 0.9966，方法检测限（LOD）在 0.005-0.02ng/mL 范围内。此外，在空白水样中添加三个浓度水平的回收率范围为 86.9-114.6%，日内和日间相对标准偏差（RSD）为 0.8-11.0%。最后，将所提出的方法成功应用于实际水样中 8 种 PCA 除草剂的提取，然后用超高效液相色谱串联质谱法（UHPLC-MS/MS）进行测定。结果表明，mOAS 作为磁性固相萃取（MSPE）酸性除草剂的吸附剂，具有简单、快速的优点，是一种有效的替代品。
